US569419A - Heinrich laubmann - Google Patents

Description

UNITED STATES PATENT OFFICE.

HEINRICH LAUBMANN, OF HOCHST-ON-THE-MAIN, GERMANY, ASSIGNOR TO THE FARBYVERKE, VORMALS MEISTER, LUCIUS d: BRHNING, OF SAME PLACE.

DiNITROANTHRACHRYSONE-DISULFONIC ACID AND METHOD OF MAKING SAME.

SPECIFICATION forming part of Letters Patent No. 569,419, dated October 13, 1896.

Application filed May 10, 1894. Serial No. 510,789. (Specimena) Patented in Germany DecemherZS, 1892,11'0. 70,806.

To all whom it may concern:

Be it known that I, HEINRICH LAUBMANN, a citizen of the Empire of Germany, residing at Hiichst-on-the-Main, in the Empire of Ger 5 many, have invented certain new and useful Improvements in the Production of Dinitroantlirachrysone-Disulfonic Acid, (for which Letters Patent were granted to me in Germany, No. 70,806, dated December 28, 1892,)

of which the following is a specification.

Anthrachrysone being treated with fuming sulfuric acid of ten to twenty per cent. at a temperature of from 100 to 120 centigrade transforms into a disulfonic acid which can quite I 5 easily be converted into a nitro product, the dinitroanthrachrysone-disulfonic acid. The production of this acid can be carried out by dissolving the free anthrachrysone-disulfonic acid in concentrated sulfuric acid and converting the same by nitration in the usual manner into the dinitro acid. A more simple way for its production is starting from the anthrachrysone, converting the same into the disulfonic acid by means of fuming sulfuric 2 5 acid and nitratin g this acid without previous insulating.

The production of the nitrosulfonic acid from anthrachrysone may, for example, be carried out in the following manner: An-

0 thrachrysone is sulfonized with its from four to five fold quantity by weight of fuming sulfuric acid from ten to twenty per cent, anhydrid at about 100 centigrade up to being soluble in water. The sulfonation mixture 3 5 after cooling down is diluted with about the equal volume of sulfuric acid of 66 Baum and while stirring well is caused slowly to flow into the quantity of nitric acid demanded by theory for two nitro groups, best in the 40 form of nitrating acid. W'hen the nitric acid has been added, the mixture is heated to about 80 centigrade for a shorttime, and after cooling down again it is poured upon ice, the solution boiled up, and filtered. The dinitroanthrachrysone-disulfonic acid separates. It is removed by filtrating, and the nitrosulfonic acid remaining in the filtrate recovered by precipitating by means of common salt. By precipitating with concentrated hydrochloric acid and washing with somewhat diluted hy- 5o drochloric acid it may be purified.

hen the nitroanthrachrysonedisulfonic acid is to be produced from the free anthrachrysone e disulfouic acid, the same is dissolved in from ten to fifteen fold its quantity 5 5 by weight of concentrated sulfuric acid of Baum and the quantity of nitric acid demanded by theory, best in form of nitrating acid, caused slowly to flow into it while stirring well. The reaction mass is then treated 60 with nitrosulfonic acid insulated and purified in manner like described in the preceding example.

The free anthrachrysone-disulfonic acid is in form of a greenish-yellow crystalline powder of easy solubility in water and alcohol, but very clifficultly soluble in glacial acetic acid, and maybe crystallized from this solution. Heated above 230 centigrade the acid undergoes rather impetuous decomposition.

In a-lkalies the dinitroanthrachrysone-disulfonic acid dissolves with red color. From this solution diluted acids precipitate an acid sodium salt which crystallizes from water in the form of beautiful gold-yellow leaflets.

The analysis gave numbers corresponding to those demanded by the formula:

C.. i0i l ii 1i t n Na 7.04 7.8 pr. s 10.8 10.9 pr. N 4 7 1.8 pr.

when the dinitroanthrachrysone-disulfonic acid is treated with reducing agencies, such as iron, zinc, &c. in an acid solution, and subsequently boiled with alkalies, a blue coloring-matter is derived of varying shades, ran ging from deep blue to violet.

hat I claim as my invention is- 1. The process of producing dinitroanthrachrysone-disulfonic acid, which consists in sulfonizing anthrachrysone, and nitrating the sulfonation product, substantially as described.

2. Asa new article of manufacture, dinitroanthrachrysone-disu1fonic acid having the following characteristics: being easily soluble in water and alcohol, quickly soluble in ether, benzin, chloroform and glacial acetic acid, undergoing rapid decomposition on being heated above 230 centigrade, soluble in alkalies with reddish color, its sodium salts crystallizing from water in the form of goldyellow leaflets which on analysis give numbers corresponding to the formula o rr o (No, ,(so,Na ,H,o.

In testimony that I claim the foregoing as my invention I have signed my name in presence of two subscribing witnesses.

HEINRICH LAUBMANN.

Vitnesses:

J OSEF REVERDY, HEINRIOH HAHN.